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NASA NTRS2003

Ultra-high Temperature Ceramic Composites for Leading Edges

Ultra-high temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTC. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHT applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTC for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The progress on approaches to improving oxidation resistance by alloying and functional grading will be reported. In particular, initial tests of tantalum additions have shown potential for major improvement. Less promising results of additional tests at higher temperatures will be presented. Two fabrication approaches are being pursued to produce carbon fiber reinforced UHTC composites: prepregging and rigid perform infiltration. Fabrication procedures and microstructures for composites will be reported.

Levine, Stanley R.↗

NASA NTRS2003

Ultra-High Temperature Ceramic Composites for Leading Edges

Ultra-high temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTC. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHTC applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTC for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The progress on approaches to improving oxidation resistance by alloying and functional grading will be reported. In particular, initial tests of tantalum additions have shown potential for major improvement. Results for additional tests at higher temperatures will be presented. These oxidation improvements are being incorporated in the composites approaches. Two fabrication approaches are being persued to produce carbon fiber reinforced UHTC composites: prepregging and rigid perform infiltration. Fabrication procedures, microstructures, and initial mechanical property and oxidation results for composites will be reported.

Levine, Stanley R.↗

NASA NTRS2004

COTS Ceramic Chip Capacitors: An Evaluation of the Parts and Assurance Methodologies

Commercial-Off-The-Shelf (COTS) multilayer ceramic chip capacitors (MLCCs) are continually evolving to reduce physical size and increase volumetric efficiency. Designers of high reliability aerospace and military systems are attracted to these attributes of COTS MLCCs and would like to take advantage of them while maintaining the high standards for long-term reliable operation they are accustomed io when selecting military qualified established reliability (MIL-ER) MLCCs. However, MIL-ER MLCCs are not available in the full range of small chip sizes with high capacitance as found in today's COTS MLCCs. The objectives for this evaluation were to assess the long-term performance of small case size COTS MLCCs and to identify effective, lower-cost product assurance methodologies. Fifteen (15) lots of COTS X7R dielectric MLCCs from four (4) different manufacturers and two (2) MIL-ER BX dielectric MLCCs from two (2) of the same manufacturers were evaluated. Both 0805 and 0402 chip sizes were included. Several voltage ratings were tested ranging from a high of 50 volts to a low of 6.3 volts. The evaluation consisted of a comprehensive screening and qualification test program based upon MIL-PRF-55681 (i.e., voltage conditioning, thermal shock, moisture resistance, 2000-hour life test, etc.). In addition, several lot characterization tests were performed including Destructive Physical Analysis (DPA), Highly Accelerated Life Test (HALT) and Dielectric Voltage Breakdown Strength. The data analysis included a comparison of the 2000-hour life test results (used as a metric for long-term performance) relative to the screening and characterization test results. Results of this analysis indicate that the long-term life performance of COTS MLCCs is variable -- some lots perform well, some lots perform poorly. DPA and HALT were found to be promising lot characterization tests to identify substandard COTS MLCC lots prior to conducting more expensive screening and qualification tests. The results indicate that lot- specific screening and qualification are still recommended for high reliability applications. One significant and concerning observation is that MIL- type voltage conditioning (100 hours at twice rated voltage, 125 C) was not an effective screen in removing infant mortality parts for the particular lots of COTS MLCCs evaluated.

Brusse, Jay A.↗

NASA NTRS2004

Ultra-high Temperature Ceramic Composites for Leading Edges, 2004

Ultrahigh temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of the UHTC. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHTC applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTC for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The progress on approaches to improving oxidation resistance by alloying and functional grading will be reported.

Levine, Stanley R.↗

NASA NTRS2004

UHTC Composites for Leading Edges

Ultrahigh temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought tot he fore by the low fracture tougness and thermal shock resistance of UHTC. In addition, poor oxidation resistance is a limitation on UHTC applicability to reusable launch vehicles. We have been addressing these deficiencies for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on UHTC composite (UHTCC) constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. Processing, mechanical property, and oxidation resutls will be reported.

Levine, Stanley R.↗

NASA NTRS1999

Thermal Mechanical Stability of Single-Crystal-Oxide Refractive Concentrators Evaluated for High-Temperature Solar-Thermal Propulsion

Recently, refractive secondary solar concentrator systems were developed for solar thermal power and propulsion (ref. 1). Single-crystal oxides-such as yttria-stabilized zirconia (Y2O3-ZrO2), yttrium aluminum garnet (Y3Al5O12, or YAG), magnesium oxide (MgO), and sapphire (Al2O3)-are candidate refractive secondary concentrator materials. However, the refractive concentrator system will experience high-temperature thermal cycling in the solar thermal engine during the sun/shade transition of a space mission. The thermal mechanical reliability of these components in severe thermal environments is of great concern. Simulated mission tests are important for evaluating these candidate oxide materials under a variety of transient and steady-state heat flux conditions. In this research at the NASA Lewis Research Center, a controlled heat flux test approach was developed for investigating the thermal mechanical stability of the candidate oxide. This approach used a 3.0-kW continuous-wave (wavelength, 10.6 mm) carbon dioxide (CO2) laser (ref. 2). The CO2 laser is especially well-suited for single-crystal thermal shock tests because it can directly deliver well-characterized heat energy to the oxide surfaces. Since the oxides are opaque at the 10.6-mm wavelength of the laser beam, the light energy is absorbed at the surfaces rather than transmitting into the crystals, and thus generates the required temperature gradients within the specimens. The following figure is a schematic diagram of the test rig.

Jacobson, Nathan S.↗

NASA NTRS2000

Affordable, Robust Ceramic Joining Technology (ARCJoinT) Given 1999 R and D 100 Award

Advanced ceramics and fiber-reinforced ceramic matrix composites with high strength and toughness, good thermal conductivity, thermal shock resistance, and oxidation resistance are needed for high-temperature structural applications in advanced high-efficiency and high-performance engines, space propulsion components, and land-based systems. The engineering designs of these systems require the manufacturing of large parts with complex shapes, which are either quite expensive or impossible to fabricate. In many instances, it is more economical to build complex shapes by joining together simple geometrical shapes. Thus, joining has been recognized as an enabling technology for the successful utilization of advanced ceramics and fiber-reinforced composite components in high-temperature applications. However, such joints must retain their structural integrity at high temperatures and must have mechanical strength and environmental stability comparable to those of the bulk materials. In addition, the joining technique should be robust, practical, and reliable. ARCJoinT, which is based on the reaction-forming approach, is unique in terms of producing joints with tailorable microstructures. The formation of joints by this approach is attractive since the thermomechanical properties of the joint interlayer can be tailored to be very close to those of the base materials. In addition, high-temperature fixturing is not needed to hold the parts at the infiltration temperature. The joining process begins with the application of a carbonaceous mixture in the joint area, holding the items to be joined in a fixture, and curing at 110 to 120 C for 10 to 20 min. This step fastens the pieces together. Then, silicon or a silicon alloy in tape, paste, or slurry form is applied around the joint region and heated to 1250 to 1425 C (depending on the type of infiltrant) for 10 to 15 min. The molten silicon or silicon-refractory metal alloy reacts with carbon to form silicon carbide with controllable amounts of silicon and other phases as determined by the alloy composition. Joint thickness can be readily controlled through adjustments of the properties of the carbonaceous paste and the applied fixturing force. The photograph shows various shapes of silicon-carbide-based ceramics and fiberreinforced composites that have been joined using ARCJoinT. Thermomechanical and thermochemical characterization of joints is underway for a wide variety of silicon-carbidebased advanced ceramics and fiber-reinforced composites under the hostile environments that will be encountered in engine applications. ARCJoinT, which was developed by researchers at the NASA Glenn Research Center at Lewis Field, received R&D Magazine's prestigious R&D 100 Award in 1999.

Singh, Mrityunjay↗

NASA NTRS2001

Transient Reliability Analysis Capability Developed for CARES/Life

The CARES/Life software developed at the NASA Glenn Research Center provides a general-purpose design tool that predicts the probability of the failure of a ceramic component as a function of its time in service. This award-winning software has been widely used by U.S. industry to establish the reliability and life of a brittle material (e.g., ceramic, intermetallic, and graphite) structures in a wide variety of 21st century applications.Present capabilities of the NASA CARES/Life code include probabilistic life prediction of ceramic components subjected to fast fracture, slow crack growth (stress corrosion), and cyclic fatigue failure modes. Currently, this code can compute the time-dependent reliability of ceramic structures subjected to simple time-dependent loading. For example, in slow crack growth failure conditions CARES/Life can handle sustained and linearly increasing time-dependent loads, whereas in cyclic fatigue applications various types of repetitive constant-amplitude loads can be accounted for. However, in real applications applied loads are rarely that simple but vary with time in more complex ways such as engine startup, shutdown, and dynamic and vibrational loads. In addition, when a given component is subjected to transient environmental and or thermal conditions, the material properties also vary with time. A methodology has now been developed to allow the CARES/Life computer code to perform reliability analysis of ceramic components undergoing transient thermal and mechanical loading. This means that CARES/Life will be able to analyze finite element models of ceramic components that simulate dynamic engine operating conditions. The methodology developed is generalized to account for material property variation (on strength distribution and fatigue) as a function of temperature. This allows CARES/Life to analyze components undergoing rapid temperature change in other words, components undergoing thermal shock. In addition, the capability has been developed to perform reliability analysis for components that undergo proof testing involving transient loads. This methodology was developed for environmentally assisted crack growth (crack growth as a function of time and loading), but it will be extended to account for cyclic fatigue (crack growth as a function of load cycles) as well.

Nemeth, Noel N.↗

NASA NTRS2002

Strength and Fracture Toughness of Solid Oxide Fuel Cell Electrolyte Material Improved

Solid oxide fuel cells (SOFC) are being developed for various applications in the automobile, power-generation, and aeronautics industries. Recently, the NASA Glenn Research Center has been exploring the possibility of using SOFC's for aeropropulsion under its Zero Carbon Dioxide Emission Technology (ZCET) Program. 10-mol% yttriastabilized zirconia (10YSZ) is a very good anionic conductor at high temperatures and is, therefore, used as an oxygen solid electrolyte in SOFC. However, it has a high thermal expansion coefficient, low thermal shock resistance, low fracture toughness, and poor mechanical strength. For aeronautic applications, the thin ceramic electrolyte membrane of the SOFC needs to be strong and tough. Therefore, we have been investigating the possibility of enhancing the strength and fracture toughness of the 10YSZ electrolyte without degrading its electrical conductivity to an appreciable extent. We recently demonstrated that the addition of alumina to zirconia electrolyte increases its strength as well as its fracture toughness. Zirconia-alumina composites containing 0 to 30 mol% of alumina were fabricated by hot pressing. The hot pressing procedure was developed and various hot pressing parameters were optimized, resulting in dense, crackfree panels of composite materials. Cubic zirconia and a-alumina were the only phases detected, indicating that there was no chemical reaction between the constituents during hot pressing at elevated temperatures. Flexure strength sf and fracture toughness K(sub IC) of the various zirconia-alumina composites were measured at room temperature as well as at 1000 C in air. Both properties showed systematic improvement with increased alumina addition at room temperature and at 1000 C. Use of these modified electrolytes with improved strength and fracture toughness should prolong the life and enhance the performance of SOFC in aeronautics and other applications.

Bansal, Narottam P.↗

NASA NTRS2004

Issues for Ultra-High Temperature Composites

Ultra-high temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTC. In addition, poor oxidation resistance is a limitation on UHTC applicability to reu'sable launch vehicles. We have been addressing these deficiencies by investigating methods for improving the oxidation resistance of UHTC and by evaluating the performance of an early polymer precursor derived UHTC composite. Processing, mechanical property, and furnace oxidation and oxyacetylene torch exposure results are reported. From these results guidelines for UHTC composite architecture, constituents, and processing are developed.

Levine, Stanley R.↗

NASA NTRS2003

Robust UHTC for Sharp Leading Edge Applications

Ultrahigh temperature ceramics have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTCs. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHTC applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTCs for the past year via a small task at GRC that is part of the 3rd Gen TPS effort. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The approaches and progress will be reported.

Levine, Stanley R.↗

NASA NTRS2003

UHTC for Sharp Leading Edges

Levine, Stanley R.↗

NASA NTRS2002

Evaluation of Ultra-High Temperature Ceramics for Propulsion Application

Ultra-high temperature ceramic (UHTC) materials consisting of zirconium diboride or hafnium diboride plus silicon carbide offer a combination of properties that make them candidates for airframe leading edges on sharp-bodied reentry vehicles. These UHTC perform well in the environment for such applications, i.e. low pressure air. The purpose of this study was to examine three of these materials under conditions more representative of a propulsion environment, i.e. higher oxygen and total pressure. Results of stren$h and fracture toughness measurements, furnace oxidation, and thermal shock exposures are presented. The poor oxidation resistance of UHTCs is the predominant factor limiting their applicability to propulsion.

Levine, Stanley R.↗

NASA NTRS2005

Lifetime Reliability Prediction of Ceramic Structures Under Transient Thermomechanical Loads

An analytical methodology is developed to predict the probability of survival (reliability) of ceramic components subjected to harsh thermomechanical loads that can vary with time (transient reliability analysis). This capability enables more accurate prediction of ceramic component integrity against fracture in situations such as turbine startup and shutdown, operational vibrations, atmospheric reentry, or other rapid heating or cooling situations (thermal shock). The transient reliability analysis methodology developed herein incorporates the following features: fast-fracture transient analysis (reliability analysis without slow crack growth, SCG); transient analysis with SCG (reliability analysis with time-dependent damage due to SCG); a computationally efficient algorithm to compute the reliability for components subjected to repeated transient loading (block loading); cyclic fatigue modeling using a combined SCG and Walker fatigue law; proof testing for transient loads; and Weibull and fatigue parameters that are allowed to vary with temperature or time. Component-to-component variation in strength (stochastic strength response) is accounted for with the Weibull distribution, and either the principle of independent action or the Batdorf theory is used to predict the effect of multiaxial stresses on reliability. The reliability analysis can be performed either as a function of the component surface (for surface-distributed flaws) or component volume (for volume-distributed flaws). The transient reliability analysis capability has been added to the NASA CARES/ Life (Ceramic Analysis and Reliability Evaluation of Structures/Life) code. CARES/Life was also updated to interface with commercially available finite element analysis software, such as ANSYS, when used to model the effects of transient load histories. Examples are provided to demonstrate the features of the methodology as implemented in the CARES/Life program.

Nemeth, Noel N.↗

NASA NTRS2003

High performance structural laminate composite material for use to 1000.degree. F. and above, apparatus for and method of manufacturing same, and articles made with same

A novel materials technology has been developed and demonstrated for providing a high modulus composite material for use to 1000.degree. F. and above. This material can be produced at 5-20% of the cost of refractory materials, and has higher structural properties. This technology successfully resolves the problem of thermal shock or ply lift, which limits traditional high temperature laminates (such as graphite/polyimide and graphite/phenolic) to temperatures of 550-650.degree. F. in thicker (0.25 and above) laminates. The technology disclosed herein is an enabling technology for the nose for the External Tank (ET) of the Space Shuttle, and has been shown to be capable of withstanding the severe environments encountered by the nose cone through wind tunnel testing, high temperature subcomponent testing, and full scale structural, dynamic, acoustic, and damage tolerance testing.

Seal, Ellis C.↗

NASA NTRS2007

Ground-Based Testing of TiB2 and Al2O3/TiB2 Response to Space Environment

Two materials, titanium diboride and an alumina/titanium diboride composite, exhibit characteristics favorable for use in multiple space applications. These characteristics include low mass (4.52 gm/cc), high strain rate impact resistance, high temperature use (3000oC M.P.), thermal and electrical conductivity, thermal shock resistance, and high visible-range reflectivity. Additionally, the presence of boron in these materials gives them the potential to shield against neutron radiation as well as charged radiation. These materials are flying on MISSE 6 to assess material changes resulting from exposure to the space environment. This study provides a preliminary, ground-based examination of these materials' interactions with individual components of the space environment, in particular atomic oxygen (AO) and neutron radiation, in order to better predict and understand post-flight results. Individual specimens are exposed to ground state AO and surface oxidation is measured. Equivalent exposures of up to 13 months show no rapid oxidation, however evidence indicates some surface oxidation occurring. Other samples are placed near a polyethylene moderated, one Ci Am/Be neutron source to determine their shielding capability. Comparisons between exposed and shielded indium foil, which is activated by transmitted neutrons, measure each material's ability to shield neutrons. Preliminary results indicate a significant shielding benefit provided by both materials.

Jefferies, Sharon A.↗

NASA NTRS2008

Quench Crucibles Reinforced with Metal

Improved crucibles consisting mainly of metal-reinforced ceramic ampules have been developed for use in experiments in which material specimens are heated in the crucibles to various high temperatures, then quenched by, for example, plunging the crucibles into water at room temperature. In a traditional quench crucible, the gap between the ampule and the metal cartridge impedes the transfer of heat to such a degree that the quench rate (the rate of cooling of the specimen) can be too low to produce the desired effect in the specimen. One can increase the quench rate by eliminating the metal cartridge to enable direct quenching of the ampule, but then the thermal shock of direct quenching causes cracking of the ampule. In a quench crucible of the present improved type, there is no gap and no metal cartridge in the traditional sense. Instead, there is an overlay of metal in direct contact with the ampule, as shown on the right side of the figure. Because there is no gap between the metal overlay and the ampule, the heat-transfer rate can be much greater than it is in a traditional quench crucible. The metal overlay also reinforces the ampule against cracking.

Holmes, Richard R.↗

NASA NTRS2008

Igniters for Liquid Oxygen/Liquid Methane Technology Development

As part of NASA's technology development of liquid methane / liquid oxygen engines for future exploration missions, two different igniters were recently studied at NASA Marshall Space Flight Center. The first igniter tested was an impinging injection, spark-initiated torch igniter, and the second was a microwave-generated plasma igniter. The purpose of the ignition tests was to define the ignition limits under vacuum conditions and characterize the transient start-up performance as a function of propellant mixture ratio (MR), mass flow rates, inlet temperatures, and pre-ignition chamber pressure. In addition, for the impinging igniter two different spark plugs were tested, and for the microwave igniter the magnetron filament warm-up time and the magnetron input power were both varied. The results gathered from these tests indicated that the impinging igniter is capable of operating over an MR range of 2 - 27, with methane and oxygen inlet temperatures as low as -161 F and -233 F, respectively. The microwave igniter was tested over an MR range of 2 - 9, with methane and oxygen inlet temperatures as low as -90 F and -200 F, respectively. The microwave igniter achieved ignition over this range, although an upper ignition limit was determined for the oxidizer mass flow rate. In general, the torch exhaust temperatures for the microwave igniter were not as high as those attained with the impinging igniter. The microwave igniter, however, was hot-fired 17 times and was still operational, whereas the impinging igniter spark plugs experienced thermal shock and erosion over nine hot-fire tests. It was concluded that for the microwave igniter better mixing of the propellants might be required in order to both raise the torch exhaust temperature and decrease the required magnetron input power, and for the impinging igniter the spark plug position within the igniter chamber should be varied in future tests to identify a more optimal location. All of the igniter tests were supported by the Propulsion & Cryogenics Advanced Development project, which is part of NASA's Exploration Technology Development Program.

Osborne, Robin J.↗